CN101945836A - Agglomerating Ferrite Material and prepare the method for agglomerating Ferrite Material - Google Patents
Agglomerating Ferrite Material and prepare the method for agglomerating Ferrite Material Download PDFInfo
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- CN101945836A CN101945836A CN2009801053925A CN200980105392A CN101945836A CN 101945836 A CN101945836 A CN 101945836A CN 2009801053925 A CN2009801053925 A CN 2009801053925A CN 200980105392 A CN200980105392 A CN 200980105392A CN 101945836 A CN101945836 A CN 101945836A
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- ferrite material
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- 239000000463 material Substances 0.000 title claims abstract description 151
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 134
- 238000000034 method Methods 0.000 title claims description 15
- 230000035699 permeability Effects 0.000 claims abstract description 62
- 230000004907 flux Effects 0.000 claims abstract description 56
- 239000000203 mixture Substances 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims description 88
- 238000005245 sintering Methods 0.000 claims description 46
- 239000002994 raw material Substances 0.000 claims description 19
- 238000000465 moulding Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 9
- 238000004804 winding Methods 0.000 description 21
- 239000011162 core material Substances 0.000 description 15
- 239000000411 inducer Substances 0.000 description 15
- 238000010298 pulverizing process Methods 0.000 description 7
- 230000035882 stress Effects 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 230000006355 external stress Effects 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 238000010125 resin casting Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
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- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides the agglomerating Ferrite Material, it is (1-x-y-z) (Li by the composition general formula with respect to 100% mass ratio
0.5Fe
0.5) OxZnOyFe
2O
3The material of zCuO, wherein x, y, z satisfy 0.14≤x≤0.19,0.48≤y＜0.5,0≤z≤0.03, add the Bi of 0.5% mass ratio to 3% mass ratio
2O
3And obtain, it is more than 200 that described material satisfies initial permeability, saturation magnetic flux density 23 ℃ be more than the 430mT and 100 ℃ for more than the 380mT, and resistivity is 10
6More than the Ω m.
Description
Technical field
The present invention relates to be used for the agglomerating Ferrite Material of the core material of winding part, be particularly related to agglomerating Ferrite Material that satisfies high initial permeability, high saturation magnetic flux density, high resistivity and preparation method thereof, wherein, above-mentioned winding part comprises antenna, transformer of employed inducer, stick antennas etc. such as power source circuit etc.
Background technology
All the time, in order to ensure and conductor between electrical isolation, the Ferrite Material that is used for the core material of winding part has adopted the Ni based ferrite material with high resistivity, wherein, above-mentioned winding part comprises the antenna, transformer of the inducer that uses in the power source circuit etc. of DC-DC transmodulator, stick antenna etc. etc.
But, the principal constituent Ni costliness of Ni based ferrite material, and magnetostriction constant is big, and therefore, its defective is that in the winding part of resin casting mold type, when making resin solidification, soft magnetic property is owing to the stress that is applied on the core changes.
As the material that does not contain expensive Ni, known have a Li based ferrite material.Therefore the magnetostriction constant of Li based ferrite material is little, even have use in the winding part of resin casting mold type etc., the feature that the velocity of variation of soft magnetic property is still little.
But, Li based ferrite material if under the high temperature more than 1000 ℃ sintering, though then can access the high initial permeability (for example more than 200) and the high saturation magnetic flux density of purposes such as suitable inducer, antenna, be difficult to obtain high resistivity (for example 10
6More than the Ω m).
For example, as agglomerating Li based ferrite material under the high temperature more than 1000 ℃, the someone has proposed the Li based ferrite material that following Irreversible circuit element is used: forming general formula is (1-x) Li
2O (the Fe of 5-2 α-x)
2O
34xZnO4yMnO4 β Bi
2O
3, satisfy 0≤α≤0.35,0≤x≤0.45,0≤y≤0.2,0≤β≤0.005, and among x, y, the β at least 2 are not zero simultaneously, and y α non-vanishing (patent documentation 1) when being zero.
Li based ferrite material about record in the patent documentation 1, usually improve characteristics such as temperature profile, loss characteristic by making its at least 2 kinds of units containing simultaneously among Zn, Mn, the Bi, and, when in oxygen and nitrogen, heat-treating repeatedly, in nitrogen, carry out a thermal treatment at least, and in oxygen, heat-treat at last, improve resistivity thus.
But according to patent documentation 1 described Li based ferrite material, though can access the above saturation magnetic flux density of 4000G (400mT), resistivity is low, is about 10
7Ω cm (10
5Ω m).In addition,, need in oxygen and nitrogen, heat-treat repeatedly, thereby have the problem that the manufacturing cycle is elongated, manufacturing cost increases in order to improve resistivity.
On the other hand, the somebody has proposed by adding Bi
2O
3Carry out Deng sintering aid and under low temperature (about 900 ℃) that sintering is resulting, its resistivity is enhanced 10
6The Li based ferrite material (patent documentation 2) that Ω m is above, still, the problem that exists initial permeability to reduce.
In addition, because Li based ferrite material has the big feature of squareness ratio, therefore, the someone studies to use it for and stores in the core material etc. always before this.But, comparing to Ni based ferrite material, there is the little problem of saturation magnetic flux density in Li based ferrite material.Therefore, need to improve the saturation magnetic flux density of Li based ferrite material, so that it is suitable for purposes such as the inducer, antenna of the good overlapping characteristic of direct current of requirement.
Patent documentation 1: the open communique of Japan's patent application " special public clear 55-27015 "
Patent documentation 2: the open communique " spy opens 2004-153197 " of Japan's patent application
Summary of the invention
Invent problem to be solved
As mentioned above, in existing Li based ferrite material, also there is not to satisfy simultaneously at present the Li based ferrite material of high initial permeability, high saturation magnetic flux density, high resistivity.
The objective of the invention is to, provide at an easy rate to be suitable as most all kinds and (the direct winding-type of the coil bobbin that requires high resistivity for example, need not to be set; Require the gapped type that under direct-current biasing magnetic field, uses of high initial permeability and high saturation magnetic flux density; Require the resin casting mold type of high resistance to stress, or the like) the Li base agglomerating Ferrite Material of core material of winding part, this material can satisfy high initial permeability, high saturation magnetic flux density and high resistivity simultaneously, and, still can have high saturation magnetic flux density even under comparatively high temps, be applied to various uses, wherein, above-mentioned winding part comprises inducer, antenna, transformer etc.
The method that is used to deal with problems
The inventor to achieve these goals, composition to Li based ferrite material has carried out wholwe-hearted research, it found that the compositing range that can satisfy high initial permeability, high saturation magnetic flux density and high resistivity simultaneously, even and confirmed in this compositing range, not implement complicated heat treatment and also can provide various characteristics good Li based ferrite material at an easy rate, thereby finished the present invention.
Agglomerating Ferrite Material of the present invention is characterized in that, is (1-x-y-z) (Li by the composition general formula with respect to 100% mass ratio
0.5Fe
0.5) OxZnOyFe
2O
3The material of zCuO, wherein x, y, z satisfy 0.14≤x≤0.19,0.48≤y＜0.5,0≤z≤0.03, add the Bi of 0.5% mass ratio to 3% mass ratio
2O
3And obtain, it is more than 200 that described material satisfies initial permeability, saturation magnetic flux density 23 ℃ be more than the 430mT and 100 ℃ for more than the 380mT, and resistivity is 10
6More than the Ω m.
The present invention is the agglomerating Ferrite Material with above-mentioned composition, it is characterized in that, average grain size is 7.5 μ m to 25 μ m.
The present invention is the agglomerating Ferrite Material with above-mentioned composition, it is characterized in that, the velocity of variation of the initial permeability under the pressure of 30MPa is in ± 5%.
The present invention is the agglomerating Ferrite Material with above-mentioned composition, it is characterized in that, the grain boundary porosity number is more than 20 in per 100 crystal grain.
The present invention is the agglomerating Ferrite Material with above-mentioned composition, it is characterized in that, the velocity of variation of the initial permeability under the pressure of 30MPa is in ± 3%.
Winding part of the present invention is characterized in that, has used the agglomerating Ferrite Material with above-mentioned composition.
The method for preparing the agglomerating Ferrite Material of the present invention is characterized in that, comprising: the preparation raw material powder is (1-x-y-z) (Li so that obtain forming general formula
0.5Fe
0.5) OxZnOyFe
2O
3The material of zCuO, wherein x, y, z satisfy 0.14≤x≤0.19,0.48≤y＜0.5,0≤z≤0.03; The described raw material powder of presintering and obtain first presintering powder; With respect to first presintering powder of 100% mass ratio, add the Bi of 0.5% mass ratio to 3% mass ratio
2O
3And obtain second presintering powder; Pulverize described second presintering powder and obtain pulverized powder; Make described pulverized powder moulding and obtain formed body; And the described formed body of sintering and obtain the agglomerating Ferrite Material.
The method for preparing the agglomerating Ferrite Material of the present invention is characterized in that, comprising: preparation raw material powder, described raw material powder are that the composition general formula with respect to 100% mass ratio is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOyFe
2O
3The material of zCuO, wherein x, y, z satisfy 0.14≤x≤0.19,0.48≤y＜0.5,0≤z≤0.03, by adding the Bi of 0.5% mass ratio to 3% mass ratio
2O
3And obtain; The described raw material powder of presintering and obtain presintering powder; Pulverize described presintering powder and obtain pulverized powder; Make described pulverized powder moulding and obtain formed body; And the described formed body of sintering and obtain the agglomerating Ferrite Material.
The present invention is the method for preparing the agglomerating Ferrite Material with above-mentioned operation, it is characterized in that, the pre-sintering temperature of the described raw material powder of presintering is 800 ℃-1200 ℃, is preferably 1000 ℃-1200 ℃.
The effect of invention
According to the present invention, can be met the agglomerating Ferrite Material of following condition, that is: initial permeability is more than 200, saturation magnetic flux density 23 ℃ be more than the 430mT and 100 ℃ for more than the 380mT, resistivity is 10
6More than the Ω m.
The core material that agglomerating Ferrite Material of the present invention is used for winding part, can on core, directly wind the line thus and do not need coil bobbin, therefore can reduce the manufacturing cost of winding part, and can realize miniaturization, wherein, above-mentioned winding part comprises antennas such as employed inducer, stick antenna, the transformers etc. such as power source circuit of DC-DC transmodulator.
Even agglomerating Ferrite Material of the present invention at high temperature still has high saturation magnetic flux density, therefore, can provide the inducer or the antenna of the cheapness of the overlapping characteristic good of direct current by in the core material that is applied to inducer or antenna.
Agglomerating Ferrite Material of the present invention is used as the core material of the winding part of resin casting mold type, and thus, magnetic permeability is little with respect to the velocity of variation of external stress, therefore can provide the soft magnetic property deviation less winding part.
According to the present invention,, therefore can provide the Li base agglomerating that satisfies above-mentioned characteristic Ferrite Material at an easy rate owing to do not need complicated heat treatment.
According to the present invention,, therefore can reduce the velocity of variation of the initial permeability of prepared agglomerating Ferrite Material because to make pre-sintering temperature be 800 ℃-1200 ℃, be preferably 1000 ℃-1200 ℃.
The simple declaration of accompanying drawing
Fig. 1 is the composition of the agglomerating Ferrite Material among the expression embodiment 1 and the chart of characteristic.
Fig. 2 is the ZnO amount in the expression agglomerating Ferrite Material and the graphic representation of the relation between initial permeability.
Fig. 3 is the graphic representation of the relation between the saturation magnetic flux density of ZnO amount in the expression agglomerating Ferrite Material and 23 ℃.
Fig. 4 is the graphic representation of the relation between the saturation magnetic flux density of ZnO amount in the expression agglomerating Ferrite Material and 100 ℃.
Fig. 5 is the ZnO amount in the expression agglomerating Ferrite Material and the graphic representation of the relation between resistivity.
Fig. 6 is the composition of the agglomerating Ferrite Material among the expression embodiment 2 and the chart of characteristic.
Fig. 7 is the Fe in the expression agglomerating Ferrite Material
2O
3The graphic representation of the relation between amount and initial permeability.
Fig. 8 is the Fe in the expression agglomerating Ferrite Material
2O
3The graphic representation of the relation between amount and 23 ℃ saturation magnetic flux density.
Fig. 9 is the Fe in the expression agglomerating Ferrite Material
2O
3The graphic representation of the relation between amount and 100 ℃ saturation magnetic flux density.
Figure 10 is the Fe in the expression agglomerating Ferrite Material
2O
3The graphic representation of the relation between amount and resistivity.
Figure 11 is the composition of the agglomerating Ferrite Material among the expression embodiment 3 and the chart of characteristic.
Figure 12 is the CuO amount in the expression agglomerating Ferrite Material and the graphic representation of the relation between initial permeability.
Figure 13 is the graphic representation of the relation between the saturation magnetic flux density of CuO amount in the expression agglomerating Ferrite Material and 23 ℃.
Figure 14 is the graphic representation of the relation between the saturation magnetic flux density of CuO amount in the expression agglomerating Ferrite Material and 100 ℃.
Figure 15 is the CuO amount in the expression agglomerating Ferrite Material and the graphic representation of the relation between resistivity.
Figure 16 is the composition of the agglomerating Ferrite Material among the expression embodiment 4 and the chart of characteristic.
Figure 17 is the Bi in the expression agglomerating Ferrite Material
2O
3The graphic representation of the relation between amount and initial permeability.
Figure 18 is the Bi in the expression agglomerating Ferrite Material
2O
3The graphic representation of the relation between amount and 23 ℃ saturation magnetic flux density.
Figure 19 is the Bi in the expression agglomerating Ferrite Material
2O
3The graphic representation of the relation between amount and 100 ℃ saturation magnetic flux density.
Figure 20 is the Bi in the expression agglomerating Ferrite Material
2O
3The graphic representation of the relation between amount and resistivity.
Figure 21 is the composition of the agglomerating Ferrite Material among the expression embodiment 5 and the chart of characteristic.
Figure 22 is the figure that organizes photo of the agglomerating Ferrite Material of expression comparative example.
Figure 23 is the figure that organizes photo of expression agglomerating Ferrite Material of the present invention.
Figure 24 is the chart of characteristic of the inducer of expression embodiment 6.
Figure 25 is the sketch chart of the structure of expression inducer.
Figure 26 is the chart of the antenna characteristics among the expression embodiment 7.
Figure 27 is the sketch chart of the structure of expression antenna.
Figure 28 is the chart of the characteristic of the agglomerating Ferrite Material among the expression embodiment 8.
Figure 29 is the graphic representation of the relation between the velocity of variation of grain boundary porosity number and initial permeability in per 100 crystal grain in the expression agglomerating Ferrite Material.
Figure 30 is the figure of the SEM photo of the pulverized powder among expression the present invention.
Figure 31 is the figure of the SEM photo of the pulverized powder among expression the present invention.
Figure 32 is the figure of the SEM photo of the pulverized powder among expression the present invention.
Figure 33 is the figure that organizes photo of expression agglomerating Ferrite Material of the present invention.
Figure 34 is the figure that organizes photo of expression agglomerating Ferrite Material of the present invention.
Figure 35 is the figure that organizes photo of expression agglomerating Ferrite Material of the present invention.
Embodiment
Agglomerating Ferrite Material of the present invention is characterized in that, it is (1-x-y-z) (Li by the composition general formula with respect to 100% mass ratio
0.5Fe
0.5) OxZnOyFe
2O
3The material of zCuO, wherein x, y, z satisfy 0.14≤x≤0.19,0.48≤y＜0.5,0≤z≤0.03, add the Bi of 0.5% mass ratio to 3% mass ratio
2O
3And obtain.
In claims of above-mentioned patent documentation 1, put down in writing the Li based ferrite material with following composition, that is: forming general formula is (1-x) Li
2O (the Fe of 5-2 α-x)
2O
34xZnO4yMnO4 β Bi
2O
3, satisfy 0≤α≤0.35,0≤x≤0.45,0≤y≤0.2,0≤β≤0.005, and among x, y, the β at least 2 are not zero simultaneously, and y when being zero α non-vanishing.
According to patent documentation 1 because " among x, y, the β at least 2 be not simultaneously zero ", therefore must contain simultaneously Mn and Zn, Zn and Bi, Mn and Bi or, Mn and Zn and Bi, in the embodiment of patent documentation 1, almost all contain Mn.Among the embodiment, the embodiment that does not contain Mn has only the specimen coding MLF-37 of the 3rd table.And,, put down in writing that " still, if y=0, promptly do not contain Mn, then direct current resistance becomes minimum and is not suitable as microwave circuit and comes practical application as the explanation of the 3rd table.”。Being scaled composition general formula of the present invention if said sample is numbered the composition of MLF-37, then is Fe
2O
3=0.5, (Li
0.5Fe
0.5) O=0.3, ZnO=0.2.
As mentioned above, do not contain MnO (except the situation of sneaking into) in the agglomerating Ferrite Material of the present invention as unavoidable impurities.In addition, be limited to 0.19 on the ZnO, Fe
2O
3The upper limit less than 0.5 (not comprising 0.5).And, as described later shown in the embodiment, though do not contain MnO among the present invention, but still can access 10
6The high resistivity that Ω m is above.The composition of agglomerating Ferrite Material of the present invention is in view of existing Li based ferrite material, and the composition of the Li based ferrite material that can satisfy high initial permeability, high saturation magnetic flux density, high resistivity has simultaneously been carried out wholwe-hearted research found.
Below, the composition of the agglomerating Ferrite Material of claim 1 of the present invention is limited reason be elaborated.
X is the containing ratio of ZnO, is preferably the scope of 0.14-0.19 (promptly 0.14 to 0.19, following "-" also represents the identical meaning).If less than 0.14, thereby then initial permeability diminishes and is lower than 200, if surpass 0.19, then saturation magnetic flux density diminishes, and is lower than 430mT, 100 ℃ at 23 ℃ and is lower than 380mT, and is therefore not preferred.Preferred scope is 0.16-0.17, can access following characteristic, that is: initial permeability is more than 250, saturation magnetic flux density 23 ℃ be more than the 440mT and 100 ℃ for more than the 400mT, resistivity is 10
6More than the Ω m.
Y is corresponding to Fe
2O
3Containing ratio, it does not comprise (Li
0.5Fe
0.5) Fe among the O, be preferably more than and equal 0.48 less than 0.5 scope, can satisfy: initial permeability is more than 200, saturation magnetic flux density 23 ℃ be more than the 430mT and 100 ℃ for more than the 380mT, resistivity is 10
6More than the Ω m.If y is less than 0.48, then saturation magnetic flux density diminishes, and is lower than 430mT at 23 ℃, is lower than 380mT at 100 ℃; If more than 0.5 then resistivity be lower than 10
6Ω m, therefore not preferred.Particularly if y be more than 0.5 then resistivity sharply reduce.Therefore, in order to obtain the preferred y of stable resistivity less than 0.5.Preferred scope is 0.485-0.495, thereby can access following characteristic: initial permeability is more than 250, saturation magnetic flux density 23 ℃ be more than the 440mT and 100 ℃ for more than the 400mT, resistivity is 10
6More than the Ω m, be suitable as the inducer or the antenna material that require the good overlapping characteristic of direct current most.In addition, (Li
0.5Fe
0.5) O is above-mentioned x, y and the surplus of z described later.
Z is the containing ratio of CuO, is preferably below 0.03 during interpolation.Among the present invention, can not access each good characteristic yet, but resistivity is further improved by adding CuO even do not add CuO.In addition, as described above, CuO is used for displacement (Li
0.5Fe
0.5) a part among the O, by the interpolation of CuO, even make Bi described later
2O
3Addition reduce and still can keep good characteristic, and by reducing Bi
2O
3Amount can play the effect that ferrite sintered body is provided at an easy rate.If z surpasses 0.03, then saturation magnetic flux density diminishes, and is lower than 430mT at 23 ℃, is lower than 380mT at 100 ℃, and is therefore not preferred.Preferred scope is below 0.02.
With respect to the material with above-mentioned composition of 100% mass ratio, add the Bi of 0.5% mass ratio-3% mass ratio
2O
3In the past, in Li based ferrite material, if the high temperature sintering that carries out more than 1000 ℃ then is difficult to obtain 10
6The resistivity that Ω m is above, but by in the material of above-mentioned composition general formula, adding the Bi of 0.5% mass ratio-3% mass ratio
2O
3Even carry out high temperature sintering and also can access high resistivity.If Bi
2O
3Less than 0.5% mass ratio, the effect of the resistivity that then can not be improved, if surpass 3% mass ratio, then saturation magnetic flux density reduces, and is therefore not preferred.Preferred scope is 0.5% mass ratio-1.25% mass ratio.In addition, in preparation method described later, preferably after the presintering operation, add Bi before the sintering circuit
2O
3
Limit reason by satisfying above-mentioned composition, can be met the agglomerating Ferrite Material of following condition, that is: initial permeability more than 200, saturation magnetic flux density be more than the 430mT and at 100 ℃ to be that resistivity is 10 more than the 380mT at 23 ℃
6More than the Ω m.In addition, agglomerating Ferrite Material of the present invention can allow unavoidable impurities.For example, though MnO is not the bioelement of agglomerating Ferrite Material of the present invention,, can't produce detrimentally affect if only limit to the degree of sneaking into as impurity.
Agglomerating Ferrite Material of the present invention can obtain by following preparation method.
At first, preparation material, this material are that the composition general formula with respect to 100% mass ratio is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOyFe
2O
3The material of zCuO, wherein x, y, z satisfy 0.14≤x≤0.19,0.48≤y＜0.5,0≤z≤0.03, by adding the Bi of 0.5% mass ratio to 3% mass ratio
2O
3And obtain.
The operation of preparation above-mentioned materials is as long as before sintering circuit described later.That is, the preparation above-mentioned materials gets final product in weighing, mixing, presintering, pulverizing, each operation of moulding.For example, at first weighing, be mixed into the carbonate powder and the oxide powder of the starting raw material of whole elements, and carry out presintering; Also only weighing, mix other raw material powder except that raw material powders such as Bi, Li and carry out presintering, in above-mentioned presintering powder, mix raw material powders such as Bi, Li then after, pulverize again, moulding.Perhaps, also can mix in the pulverized powder after pulverizing, and then carry out sintering.
In the presintering operation, pre-sintering temperature is preferably 800 ℃-1200 ℃.More preferably 1000 ℃-1200 ℃.Heat above-mentioned mixing raw material powder by the presintering operation, and form the ferrite phase by solid state reaction (ferrite reaction).The presintering time was preferably 2 hours-5 hours.In addition, presintering atmosphere is preferably in the atmosphere or in the oxygen.
Agglomerating Ferrite Material of the present invention is characterised in that to have good initial permeability, saturation magnetic flux density, resistivity, and initial permeability is little with respect to the velocity of variation of external stress.Utilize above-mentioned compositing range, carry out presintering and via operation described later at 800 ℃-1200 ℃, the velocity of variation that obtains the initial permeability under the pressure of 30MPa thus is for ± 5% with interior agglomerating Ferrite Material, by under the higher temperature of 1000 ℃-1200 ℃ ratio, carrying out presintering, initial permeability is reduced with respect to the velocity of variation of external stress, thereby the velocity of variation that can access the initial permeability under the pressure of 30MPa is for ± 3% with interior agglomerating Ferrite Material.
If under the higher temperature of 1000 ℃-1200 ℃ ratio, carry out presintering, form neck between the powder after then the ferrite reaction finishes, carry out combination between powder.Therefore, becoming in pulverizing process described later is difficult to be pulverized, and becomes the pulverized powder that contains big powder and less powder, that is, so-called size distribution curve is not sharp-pointed.
With this pulverized powder moulding, sintering, the number of pores that forms on the crystal boundary is increased, and external stress is relaxed, therefore initial permeability is further reduced with respect to the velocity of variation of external stress.
In pulverizing process, pulverize and preferably in pure water or ethanol, carry out.In addition, the median size of the pulverized powder after the pulverizing is preferably 0.5 μ m-2.0 μ m.
Pulverized powder after the pulverizing carries out moulding by required forming method.Before the moulding, can carry out granulation by prilling granulator to pulverized powder as required.Forming pressure is preferably 70MPa-150MPa.
The formed body that obtains by aforesaid operations is carried out sintering, obtain the agglomerating Ferrite Material.Sintering temperature is preferably 1000-1150 ℃.If be lower than 1000 ℃ then initial permeability reduce, if surpass 1150 ℃ of then Bi distillations in the formed body and exist and pollute the possibility that waits in the stove, therefore not preferred.Preferred scope is 1050 ℃-1100 ℃.Preferably in atmosphere or in the oxygen, sintering time is preferably 2-5 hour to sintering atmosphere.
Agglomerating Ferrite Material of the present invention can improve initial permeability and saturation magnetic flux density and resistivity is reduced by the average grain size behind the sintering being adjusted into 7.5 μ m to 25 μ m.It has been generally acknowledged that,, preferably reduce average grain size and grain boundary resistance is increased in order to obtain high resistivity.But can be confirmed by agglomerating Ferrite Material of the present invention: when average grain size during greater than the average grain size of current material, initial permeability and saturation magnetic flux density are improved and can't cause resistivity to reduce.Can think that this effect owing to the compositing range of agglomerating Ferrite Material of the present invention, is an intrinsic effect of the present invention.
By making average grain size is more than the 7.5 μ m, and the effect of the initial permeability that can be improved and saturation magnetic flux density is therefore preferred.If surpass 25 μ m, then resistivity reduces, and is therefore not preferred.Average grain size can be adjusted by above-mentioned pre-sintering temperature/time, powder particle diameter, sintering temperature/time.
Embodiment
(embodiment 1)
The composition of verifying x (ZnO) by present embodiment limits reason.
Carbonate powder and the oxide powder that becomes starting raw material carried out weighing, mixing, make final to consist of various compositions shown in Figure 1 (in following whole embodiment, about (the Li of each figure
0.5Fe
0.5) O, ZnO, Fe
2O
3, CuO carries out mark with mol%.Form x, y in the general formula, z 0.01 corresponding to 1mol%), and 1000 ℃ of following presintering obtained presintering powder (first presintering powder) in 3 hours in atmosphere.Add the Bi of 0.75% mass ratio with respect to the presintering powder (first presintering powder) of the gained of 100% mass ratio
2O
3Obtain presintering powder (second presintering powder).By ball mill this presintering powder (second presintering powder) is carried out case of wet attrition and make its grain-size reach 0.5 μ m to 2 μ m, carry out drying then.
In the powder of gained, add the polyvinyl alcohol of 1% weight ratio, carry out granulation and make prilling powder, at the forming pressure compacted under of 150MPa is the frame shape of tabular and housing 9.5mm * inside casing 4.7mm * thick 2.4mm of the ring-type of external diameter 9mm * internal diameter 4mm * thick 3mm and 30mm * 20mm * thick 5mm, the formed body to gained carries out 3 hours sintering under 1050 ℃ in atmosphere, obtains the agglomerating Ferrite Material.
Ring-type agglomerating Ferrite Material to gained is implemented coiling, measures initial permeability with f=100kHz in room temperature (23 ℃) by LCR survey meter (HEWLETT PACKARD makes, device name 4285A).In addition, measure the BP circulation of 4000A/m.Measurement result is shown in Fig. 1.
In addition, cut out the sample of 17mm * 2mm * thick 2mm,, measure the resistance of sample in room temperature (23 ℃) by the two-terminal method at two ends coating conductive paste from the tabular agglomerating Ferrite Material of gained.Measurement result is shown in Fig. 1.In addition, in each following figure, in the following manner electricalresistivity's (Ω m) value is carried out mark, for example, if be 24 * 10
7Then it is labeled as 2.4E+07.
In addition, the agglomerating Ferrite Material of the frame shape of gained is implemented coiling, measure initial permeability by LCR survey meter same as described above.In addition, 30MPa pressurizes with single shaft, obtains the velocity of variation of the initial permeability of pressurization front and back.Measurement result is shown in Fig. 1.
In addition, in Fig. 1, specimen coding sideband " * " mark be comparative example (implication of following " * " is identical therewith).In addition, the result with Fig. 1 is depicted as graphic representation and is shown in Fig. 2-Fig. 5.Transverse axis is the ZnO amount, Fig. 2 is the graphic representation of the variation of expression initial permeability (μ i), Fig. 3 is the graphic representation of the variation of the saturation magnetic flux density (Bs) when representing 23 ℃, Fig. 4 is the graphic representation of the variation of the saturation magnetic flux density (Bs) when representing 100 ℃, and Fig. 5 is the graphic representation of the variation of expression resistivity (ρ).
By Fig. 1-Fig. 5 obviously as can be known, when in the scope of containing ratio at 0.14-0.19 of ZnO, can access good characteristic, that is: initial permeability is more than 200, saturation magnetic flux density 23 ℃ be more than the 430mT and 100 ℃ for more than the 380mT, resistivity is 10
6More than the Ω m.In addition, by the result of Fig. 1 as can be known, the initial permeability that is caused by stress of agglomerating Ferrite Material of the present invention changes less.
(embodiment 2)
By present embodiment checking y (Fe
2O
3) composition limit reason.
Final composition uses various compositions shown in Figure 6, and in addition, experiment condition is identical with embodiment 1.It is the results are shown in Fig. 6.In addition, the result with Fig. 6 is depicted as curve and is shown in Fig. 7-Figure 10.Transverse axis is Fe
2O
3Amount, Fig. 7 is the graphic representation of the variation of expression initial permeability, and Fig. 8 is the graphic representation of the variation of the saturation magnetic flux density when representing 23 ℃, and Fig. 9 is the graphic representation of the variation of the saturation magnetic flux density when representing 100 ℃, and Figure 10 is the graphic representation of the variation of expression resistivity.
By Fig. 6-Figure 10 obviously as can be known, work as Fe
2O
3Containing ratio more than or equal to 0.48 less than 0.5 scope in the time, can access good characteristic, that is: initial permeability is more than 200, saturation magnetic flux density 23 ℃ be more than the 430mT and 100 ℃ for more than the 380mT, resistivity is 10
6More than the Ω m.In addition, by the result of Fig. 6 as can be known, the initial permeability that is caused by stress of agglomerating Ferrite Material of the present invention changes less.
(embodiment 3)
Composition by present embodiment checking z (CuO) limits reason.
Final composition uses various compositions shown in Figure 11, and in addition, experiment condition is identical with embodiment 1.It is the results are shown in Figure 11.In addition, the result with Figure 11 is depicted as curve and is shown in Figure 12-Figure 15.Transverse axis is the CuO amount, Figure 12 is the graphic representation of the variation of expression initial permeability, Figure 13 is the graphic representation of the variation of the saturation magnetic flux density when representing 23 ℃, and Figure 14 is the graphic representation of the variation of the saturation magnetic flux density when representing 100 ℃, and Figure 15 is the graphic representation of the variation of expression resistivity.
By Figure 11-Figure 15 obviously as can be known, when the containing ratio of CuO is 0.03 when following, can access good characteristic, that is: initial permeability is more than 200, saturation magnetic flux density 23 ℃ be more than the 430mT and 100 ℃ for more than the 380mT, resistivity is 10
6More than the Ω m.Particularly, by Figure 15 obviously as can be known, owing to added CuO, so resistivity is improved.In addition, by the result of Figure 11 as can be known, the initial permeability that is caused by stress of agglomerating Ferrite Material of the present invention changes less.
(embodiment 4)
By present embodiment checking Bi
2O
3The qualification reason of addition.
Final composition uses various compositions shown in Figure 16, and in addition, experiment condition is identical with embodiment 1.It is the results are shown in Figure 16.In addition, the result with Figure 16 is depicted as curve and is shown in Figure 17-Figure 20.Transverse axis is Bi
2O
3Amount, Figure 17 is the graphic representation of the variation of expression initial permeability, Figure 18 is the graphic representation of the variation of the saturation magnetic flux density when representing 23 ℃, and Figure 19 is the graphic representation of the variation of the saturation magnetic flux density when representing 100 ℃, and Figure 20 is the graphic representation of the variation of expression resistivity.
By Figure 16-Figure 20 obviously as can be known, work as Bi
2O
3Addition in the scope of 0.5% mass ratio to 3% mass ratio the time, can access good characteristic, that is: initial permeability is more than 200, saturation magnetic flux density 23 ℃ be more than the 430mT and 100 ℃ for more than the 380mT, resistivity is 10
6More than the Ω m.In addition, by the result of Figure 16 as can be known, the initial permeability that is caused by stress of agglomerating Ferrite Material of the present invention changes less.
(embodiment 5)
Verify the qualification reason of the average grain size of agglomerating Ferrite Material by present embodiment.
Final composition uses composition shown in Figure 21, pre-sintering temperature is in the scope of 800 ℃ (specimen codings 28), 835 ℃ (specimen coding 29), 900 ℃ (specimen coding 30), 1000 ℃ (specimen coding 31), 1100 ℃ (specimen codings 32), in addition, experiment condition is identical with embodiment 1.Wherein, having only the sintering temperature of specimen coding 28 is 930 ℃.It is the results are shown in Figure 21.In addition, the photo of organizing with the agglomerating Ferrite Material of gained is shown in Figure 22, Figure 23.Figure 22 is the photo of organizing of specimen coding 28, and Figure 23 is the photo of organizing of specimen coding 31.
By Figure 21 obviously as can be known, by average grain size being adjusted into 7.5 μ m to 25 μ m, having improved initial permeability and saturation magnetic flux density and do not cause resistivity to reduce.
(embodiment 6)
Application examples when being applied to inducer by present embodiment checking agglomerating Ferrite Material.
Use shown in Figure 24, saturation magnetic flux density in the time of 100 ℃ as the agglomerating Ferrite Material of the present invention more than the 380mT (specimen coding 33,34) and saturation magnetic flux density agglomerating Ferrite Material of the present invention (specimen coding 35,36) 100 ℃ the time less than 380mT, made the cydariform core that inducer shown in Figure 25 is used.Core respectively be of a size of A=8.0mm, B=4.0mm, C=3.0mm, D=0.8mm, E=2.4mm, F=0.8mm.Coating copper cash 100 circles of coiling Φ 0.14mm on these cores use LCR survey meter (HEWLETT PACKARD makes, device name 4285A), under the condition determination of 100kHz, 0.1V, and the overlapping characteristic of direct current when measuring 100 ℃.In addition, according to the overlapping characteristic of direct current, obtain the current value I (A) that satisfies Δ L/L0=-10%, wherein, the inductance when L0 is I=0A, L1 are the inductance of direct current when overlapping, and Δ L represents L1-L0.Measurement result is shown in Figure 24.
By Figure 24 obviously as can be known, agglomerating Ferrite Material of the present invention has good saturation magnetic flux density, is more than the 380mT in the time of 100 ℃, and therefore, when L reduced by 10%, current value is higher to be more than the 0.5A, the overlapping characteristic good of direct current.Therefore, in the winding part that agglomerating Ferrite Material of the present invention is applied to inducer etc., can provide the inducer of the cheapness of the overlapping characteristic good of direct current.
(embodiment 7)
Application examples when the agglomerating Ferrite Material being applied to antenna by the present embodiment checking.
Use shown in Figure 26, saturation magnetic flux density in the time of 100 ℃, to be the agglomerating Ferrite Material of the present invention more than the 380mT (specimen coding 37,38) and saturation magnetic flux density agglomerating Ferrite Material of the present invention (specimen coding 39,40) 100 ℃ the time less than 380mT, make the antenna prism-shaped core of 50mm * 4mm * 4mm shown in Figure 27, coating copper cash 70 circles of coiling Φ 0.29mm on this core.Use LCR survey meter (HEWLETT PACKARD makes, a device name 4285A), under the condition determination of 100kHz, 0.1V, the overlapping characteristic of direct current when measuring 100 ℃ of winding part of gained.In addition, according to the overlapping characteristic of direct current, obtain the current value I (A) that satisfies Δ L/L0=-10%, wherein, the inductance when L0 is I=0A, L1 are the inductance of direct current when overlapping, and Δ L represents L1-L0.Measurement result is shown in Figure 26.
In addition, by determinator (the logical corporate system high temperature groove SY8232 of rock and SY8243, external amplifier NF4930), under the condition determination of 1 winding method, 10kHz, Iac=1.5A (0-peak), measure the large amplitude characteristic of above-mentioned winding part, the L temperature variation when obtaining real work.Measurement result is shown in Figure 26.
By Figure 26 obviously as can be known, agglomerating Ferrite Material of the present invention has good saturation magnetic flux density, is more than the 380mT at 100 ℃, and therefore, current value is higher for more than the 1.0A when L reduces by 10%, the overlapping characteristic good of direct current.Therefore in addition, the L temperature variation during real work is below 1.0%, even the L temperature variation is still minimum under high electric current, is suitable for the winding part as antenna etc.
(embodiment 8)
Carbonate powder and the oxide powder that becomes starting raw material carried out weighing, mixing, with the composition shown in the specimen coding 4 that obtains Fig. 1, in atmosphere, difference presintering is 3 hours under 800 ℃ of pre-sintering temperatures (specimen coding 41), 900 ℃ (specimen coding 42), 950 ℃ (specimen coding 43), 1000 ℃ (specimen coding 44), 1100 ℃ (specimen coding 45), 1200 ℃ (specimen coding 46), obtains presintering powder (first presintering powder).Add the Bi of 0.75% mass ratio with respect to the gained presintering powder (first presintering powder) of 100% mass ratio
2O
3, obtain presintering powder (second presintering powder).By ball mill with this presintering powder (second presintering powder) case of wet attrition make its grain-size be 1.1 μ m to 1.3 μ m (measuring) by air permeability method, carry out drying then.
In the powder of gained, add the polyvinyl alcohol of 1% weight ratio, carry out granulation and make prilling powder, under the forming pressure of 150MPa, carry out moulding, and in atmosphere, under 1100 ℃ of temperature the gained formed body is carried out 3 hours sintering, obtain the agglomerating Ferrite Material.
Obtain the velocity of variation of the initial permeability of agglomerating Ferrite Material under 30MPa pressure of gained.Measuring method is identical with embodiment 1.It is the results are shown in Figure 28.In addition, with the figure of curve plotting as a result of Figure 28 and be shown in Figure 29.In addition,, existing number of pores in the crystal boundary in the zone that has 100 crystal grain is counted, thereby obtained among Figure 28 grain boundary porosity number in per 100 crystal grain organizing in the photo of agglomerating Ferrite Material cross section.
By Figure 28 and Figure 29 obviously as can be known, along with pre-sintering temperature increases, the grain boundary porosity number increases, and accompanies therewith, and the velocity of variation of initial permeability diminishes.In addition as can be known, as long as pre-sintering temperature is in 800 ℃-1200 ℃ scope, the velocity of variation of initial permeability is all in ± 5%, by pre-sintering temperature being set at 1000 ℃-1200 ℃, the grain boundary porosity number reaches more than 20 in per 100 crystal grain, and it is minimum in ± 3% that the velocity of variation of initial permeability becomes.
Figure 30-Figure 32 is the SEM photo of pulverized powder, Figure 33-Figure 35 be behind the sintering the agglomerating Ferrite Material organize photo, Figure 30, Figure 33 represent the situation of specimen coding 41 (800 ℃ of pre-sintering temperatures), Figure 31, Figure 34 represent the situation of specimen coding 44 (1000 ℃ of pre-sintering temperatures), and Figure 32, Figure 35 represent the situation of specimen coding 46 (1200 ℃ of pre-sintering temperatures).
By Figure 30-Figure 32 as can be known, though the mean particle size of each pulverized powder roughly the same (1.1 μ m-1.3 μ m), the size-grade distribution difference.Can be inferred that by Figure 30 (800 ℃ of pre-sintering temperatures) size ratio of powder is consistent, size distribution curve is sharp-pointed; And can infer that by Figure 31 (1000 ℃ of sintering temperatures) and Figure 32 (1200 ℃ of sintering temperatures) contain a large amount of big powder and less powder in the powder, size distribution curve is not sharp-pointed.
As mentioned above, in sintering circuit, when under 1000 ℃ of-1200 ℃ of higher temperature, carrying out presintering, form neck between the powder after the ferrite reaction finishes, carry out combination between powder.Therefore, in pulverizing process described later, be difficult to it is pulverized.By carrying out moulding, sintering to containing a large amount of above-mentioned big powder and less powder and the not sharp-pointed pulverized powder of size distribution curve, can access the agglomerating Ferrite Material shown in Figure 34 (1000 ℃ of pre-sintering temperatures) and Figure 35 (1200 ℃ of pre-sintering temperatures), promptly, in this agglomerating Ferrite Material, the grain boundary porosity number reaches more than 20 in per 100 crystal grain, and the velocity of variation of initial permeability is minimum to be in ± 3%.In addition, in Figure 33 (800 ℃ of pre-sintering temperatures), average grain size is 11.5 μ m, also belongs in the scope of preferred average grain size of the present invention, and the velocity of variation of initial permeability is in ± 5%.
The industry utilizability
The Ferrite Material of sintering of the present invention is suitable as all kinds most (for example, does not need to arrange the direct winding-type of the bobbin that requires high resistivity; Require the gapped type that under Dc bias magnetic field, uses of high initial permeability and saturated high magnetic flux density; Require the resin casting mold type of high resistance to stress, etc.) the core material of winding part, wherein, above-mentioned winding part comprises inductor, antenna, transformer etc.
Claims (10)
1. agglomerating Ferrite Material, it is (1-x-y-z) (Li by the composition general formula with respect to 100% mass ratio
0.5Fe
0.5) OxZnOyFe
2O
3The material of zCuO, wherein x, y, z satisfy 0.14≤x≤0.19,0.48≤y＜0.5,0≤z≤0.03, add the Bi of 0.5% mass ratio to 3% mass ratio
2O
3And obtain, it is more than 200 that described material satisfies initial permeability, saturation magnetic flux density 23 ℃ be more than the 430mT and 100 ℃ for more than the 380mT, and resistivity is 10
6More than the Ω m.
2. agglomerating Ferrite Material as claimed in claim 1, wherein average grain size is 7.5 μ m to 25 μ m.
3. agglomerating Ferrite Material as claimed in claim 1 or 2, wherein the velocity of variation of the initial permeability under the pressure of 30MPa is in ± 5%.
4. agglomerating Ferrite Material as claimed in claim 1 or 2, the grain boundary porosity number is more than 20 in wherein per 100 crystal grain.
5. agglomerating Ferrite Material as claimed in claim 4, wherein the velocity of variation of the initial permeability under the pressure of 30MPa is in ± 3%.
6. use the wire wound mponent of the described agglomerating Ferrite Material of arbitrary claim among the claim 1-5.
7. prepare the method for agglomerating Ferrite Material, it comprises:
The preparation raw material powder is (1-x-y-z) (Li so that obtain forming general formula
0.5Fe
0.5) OxZnOyFe
2O
3The material of zCuO, wherein x, y, z satisfy 0.14≤x≤0.19,0.48≤y＜0.5,0≤z≤0.03;
The described raw material powder of presintering and obtain first presintering powder;
With respect to first presintering powder of 100% mass ratio, add the Bi of 0.5% mass ratio to 3% mass ratio
2O
3And obtain second presintering powder;
Pulverize described second presintering powder and obtain pulverized powder;
Make described pulverized powder moulding and obtain formed body; And
The described formed body of sintering and obtain the agglomerating Ferrite Material.
8. prepare the method for agglomerating Ferrite Material, it comprises:
Preparation raw material powder, described raw material powder are that the composition general formula with respect to 100% mass ratio is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOyFe
2O
3The material of zCuO, wherein x, y, z satisfy 0.14≤x≤0.19,0.48≤y＜0.5,0≤z≤0.03, by adding the Bi of 0.5% mass ratio to 3% mass ratio
2O
3And obtain;
The described raw material powder of presintering and obtain presintering powder;
Pulverize described presintering powder and obtain pulverized powder;
Make described pulverized powder moulding and obtain formed body; And
The described formed body of sintering and obtain the agglomerating Ferrite Material.
9. as claim 7 or the 8 described methods that prepare the agglomerating Ferrite Material, wherein the pre-sintering temperature of the described raw material powder of presintering is 800 ℃-1200 ℃.
10. the method for preparing the agglomerating Ferrite Material as claimed in claim 9, wherein said pre-sintering temperature are 1000 ℃-1200 ℃.
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| JP2009-009517 | 2009-01-20 | ||
| JP2009009517A JP5387947B2 (en) | 2008-02-14 | 2009-01-20 | Sintered ferrite material |
| PCT/JP2009/052365 WO2009101999A1 (en) | 2008-02-14 | 2009-02-13 | Sintered ferrite material and a method for the production of sintered ferrite material |
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| CN112456993A (en) * | 2020-10-29 | 2021-03-09 | 中国航天时代电子有限公司 | Microwave ferrite material for ferrite device and preparation method thereof |
| CN113213908A (en) * | 2021-04-25 | 2021-08-06 | 中国航天时代电子有限公司 | Microwave ferrite material for ferrite device and preparation method thereof |
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| US3640867A (en) * | 1968-05-10 | 1972-02-08 | Hitachi Ltd | Lithium-zinc ferrite composition with arsenic oxide or bismuth oxide additive |
| US3630912A (en) * | 1969-10-03 | 1971-12-28 | Ampex | Lithium titanium bismuth ferrites |
| JPS5297000A (en) | 1976-02-10 | 1977-08-15 | Tohoku Metal Ind Ltd | Lithium system ferrite |
| JPS5527015A (en) | 1978-08-14 | 1980-02-26 | Denki Kagaku Kogyo Kk | Preparation of catalyst solution |
| JPS6076106A (en) * | 1983-01-14 | 1985-04-30 | エヌ・ベ−・フイリツプス・フル−イランペンフアブリケン | Magnetic core |
| JP2004153197A (en) | 2002-11-01 | 2004-05-27 | Koa Corp | Magnetic material and its producing process |
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| JP2006282440A (en) * | 2005-03-31 | 2006-10-19 | Neomax Co Ltd | Oxide magnetic material |
| JP2006344683A (en) * | 2005-06-07 | 2006-12-21 | Neomax Co Ltd | Drum core and inductor |
| WO2007032338A1 (en) * | 2005-09-13 | 2007-03-22 | Hitachi Metals, Ltd. | Ferrite material |
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| CN112041951A (en) * | 2019-01-31 | 2020-12-04 | 杰富意化学株式会社 | MnCoZn-based ferrite and method for producing same |
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| US9434622B2 (en) | 2016-09-06 |
| EP2258671A1 (en) | 2010-12-08 |
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| JP2009215152A (en) | 2009-09-24 |
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